CN103456603B - Gallium system heterogeneous semiconductor substrate is prepared method and the gallium oxide film of gallium oxide film - Google Patents
Gallium system heterogeneous semiconductor substrate is prepared method and the gallium oxide film of gallium oxide film Download PDFInfo
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- CN103456603B CN103456603B CN201310401102.XA CN201310401102A CN103456603B CN 103456603 B CN103456603 B CN 103456603B CN 201310401102 A CN201310401102 A CN 201310401102A CN 103456603 B CN103456603 B CN 103456603B
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Abstract
The invention provides a kind of on gallium system heterogeneous semiconductor substrate, prepare gallium oxide film method and gallium oxide film, the method that gallium system heterogeneous semiconductor substrate is prepared gallium oxide film comprises the following steps: choose gallium based semiconductor substrate, and clears up gallium based semiconductor substrate surface; Then containing in the atmosphere of partial pressure of oxygen, external energy is adopted to process gallium based semiconductor substrate, the chemical bond that the gallium atom of gallium based semiconductor substrate surface area and other constituent atoms are formed is opened, the oxygen atom of gallium atom in atmosphere is combined and forms gallium oxygen key; Finally adopt gallium oxide film growing technology gallium based semiconductor Grown gallium oxide film after treatment.The present invention prepare on gallium system heterogeneous semiconductor substrate gallium oxide film method step science, rationally, solve the problems of prior art, effectively reduce the defect concentration of heteroepitaxial growth gallium oxide film.
Description
Technical field
The present invention relates to semi-conducting material technology of preparing, particularly relate to a kind of on gallium system heterogeneous semiconductor substrate, prepare gallium oxide film method and gallium oxide film.
Background technology
Gallium oxide material has monoclinic form, has direct band gap structure, and energy gap is 4.9eV, and in luminescence, detection and electronic device etc., have important application, be the study hotspot in current wide bandgap semiconductor materials field.Although can prepare gallium oxide single crystal in the lab at present, its crystal mass need to improve, and gallium oxide single crystal volume prepared by current laboratory is often very little, and preparation cost is very high; The gallium oxide film that what is more important is prepared in gallium oxide homogeneity single crystalline substrate is difficult to carry out combination collocation with other semi-conducting material, and this just significantly limit the application of gallium oxide film.
In order to solve the problem, people attempt by gallium oxide film preparation on other heterogeneous semiconductor substrate, and the substrate often adopted at present comprises sapphire, magnesium oxide and silicon etc.But, these substrates are different from the crystal formation of gallium oxide material, and lattice mismatch is large, causes producing larger stress at gallium oxide film in epitaxial process, the release of stress can introduce a large amount of defects in the gallium oxide film of heteroepitaxial growth, causes the quality of gallium oxide film significantly to decline.So, a kind of urgently method preparing high-quality gallium oxide film on gallium system heterogeneous semiconductor substrate.
Summary of the invention
The object of the invention is to, existingly on gallium system heterogeneous semiconductor substrate, prepare gallium oxide film for above-mentioned there is second-rate problem, propose a kind of method preparing gallium oxide film on gallium system heterogeneous semiconductor substrate, the method can be reduced in the defect concentration caused by stress in gallium oxide film effectively.
For achieving the above object, the technical solution used in the present invention is: a kind of method preparing gallium oxide film on gallium system heterogeneous semiconductor substrate, comprises the following steps:
1) choose gallium based semiconductor substrate, and clear up gallium based semiconductor substrate surface;
2) containing in the atmosphere of partial pressure of oxygen, external energy is adopted to process gallium based semiconductor substrate, the chemical bond that the gallium atom of gallium based semiconductor substrate surface area and other constituent atoms are formed is opened, the oxygen atom of gallium atom in atmosphere is combined and forms gallium oxygen key.
3) gallium oxide film growing technology gallium based semiconductor Grown gallium oxide film is after treatment adopted.
Further, described cleaning gallium based semiconductor substrate surface is the organic and inorganic impurity removing the absorption of gallium based semiconductor substrate surface, and the compound layer that substrate surface covers because of reaction.
Further, described manner of cleaning up comprises chemical cleaning and/or physical cleaning.
Further, described energy is one or more in ion beam bombardment, high energy particle irradiation, electromagnetic field and thermal radiation.
Further, described step 2) temperature is 50-1200 DEG C, air pressure is 10
-2-10
3torr, time is 1-120min, the intensity of energy is equivalent to as each gallium atom of substrate surface provides energy 10
-1-10
2eV.
Further, described gallium oxide film growing technology is the gallium oxide film growing technology of controlled extension speed.
Further, the control precision of the gallium oxide film growing technology of described controlled extension speed reaches atomic layer rank.
Further, described gallium oxide film growing technology is the one in magnetron sputtering, atomic layer epitaxy, molecular beam epitaxy and metal-organic chemical vapor deposition equipment technology.
Further, the temperature of described step 3) is 300-1200 DEG C, reative cell air pressure is 10
-9-10
3torr, oxygen source are 10 with the molar flow ratio in gallium source
-1-10
5.
Another object of the present invention also discloses a kind of gallium oxide film, and this gallium oxide film has excellent crystalline quality.
For achieving the above object, the technical solution used in the present invention is: a kind of gallium oxide film adopts the above-mentioned method preparing gallium oxide film on gallium system heterogeneous semiconductor substrate to be prepared from.
The present invention relates to the method preparing gallium oxide film on gallium system heterogeneous semiconductor substrate, first to the modifying surface area structure process again of selected substrate before growth, utilize the gallium atom in substrate, by pretreating process previously prepared skim gallium oxide film on gallium system heterogeneous semiconductor substrate.Surface-treated substrate is used to carry out subsequently epitaxial growing gallium oxide film, homogenous growth effect can be reached, can effectively reduce the defect concentration caused by stress in gallium oxide film due to lattice mismatch in heteroepitaxy, this gallium oxide film prepared can well and other semi-conducting material carry out combination collocation, make gallium oxide film can have more wide application.
Accompanying drawing explanation
Fig. 1 utilizes oxygen ion beam to the schematic diagram of gallium nitride/sapphire compound substrate modifying surface structure again in embodiment 1;
Fig. 2 be adopt metal-organic chemical vapor deposition equipment technology to cross at surface modification in embodiment 1 substrate on carry out the schematic diagram of gallium oxide film extension;
Fig. 3 is the X-ray diffraction test collection of illustrative plates of the gallium oxide film of preparation in embodiment 1;
Fig. 4 utilizes heat radiation method to the schematic diagram of gallium nitride/sapphire compound substrate modifying surface structure again in embodiment 2;
Fig. 5 adopts metal-organic chemical vapor deposition equipment technology to cross schematic diagram substrate carrying out gallium oxide film extension at surface modification in embodiment 2;
Fig. 6 is the X-ray diffraction test collection of illustrative plates of the gallium oxide film of preparation in embodiment 2.
Embodiment
The invention discloses a kind of method preparing gallium oxide film on gallium system heterogeneous semiconductor substrate, the method can be reduced in the defect concentration caused by stress in gallium oxide film due to lattice mismatch in heteroepitaxy process effectively.Particularly, the method that the present invention prepares gallium oxide film on gallium system heterogeneous semiconductor substrate comprises the following steps:
1) choose gallium based semiconductor substrate, and clear up gallium based semiconductor substrate surface;
2) in the atmosphere (atmosphere namely containing oxygen atom) containing partial pressure of oxygen, external energy is adopted to process gallium based semiconductor substrate, the chemical bond that the gallium atom of gallium based semiconductor substrate surface area and other constituent atoms are formed is opened, the oxygen atom of gallium atom in atmosphere is combined and forms gallium oxygen key.
3) gallium oxide film growing technology gallium based semiconductor Grown gallium oxide film is after treatment adopted.
Described cleaning gallium based semiconductor substrate surface is the organic and inorganic impurity removing the absorption of gallium based semiconductor substrate surface.Manner of cleaning up of the present invention comprises chemical cleaning and/or physical cleaning.
Described energy is one or more in ion beam bombardment, high energy particle irradiation, electromagnetic field and thermal radiation.
Described step 2) regulation and control process temperature be 50-1200 DEG C, be preferably 650-950 DEG C; Air pressure is 10
-2-10
3torr, is preferably 1-5torr or 760torr; Time is 1-120min, is preferably 5-30min; The intensity of energy flow energy is equivalent to as each gallium atom of substrate surface provides energy 10
-1-10
2eV, is preferably 10-20eV.The present invention comes the degree of crystallinity of controlled oxidization gallium thin layer, stoichiometric proportion, surface topography and thickness by the intensity of the temperature of regulation and control process, air pressure, time and energy.Described gallium oxide film growing technology is the gallium oxide film growing technology of controlled extension speed.The control precision of the gallium oxide film growing technology of described controlled extension speed reaches atomic layer rank.Described gallium oxide film growing technology is the one in magnetron sputtering, atomic layer epitaxy, molecular beam epitaxy and metal-organic chemical vapor deposition equipment technology.
The temperature of described step 3) is 300-1200 DEG C, is preferably 650-900 DEG C; Reative cell air pressure is 10
-9-10
3torr, is preferably 10
-9-10
-7torr or 1-5torr oxygen source is 10 with the molar flow ratio in gallium source
-1-10
5, be preferably 1-100 or 5.0 × 10
3-5.0 × 10
4.The present invention realizes the preparation of high-quality gallium oxide film by optimizing temperature, reative cell air pressure, source supply mode and quantity delivered.
The invention also discloses a kind of gallium oxide film, this gallium oxide film adopts the above-mentioned method preparing gallium oxide film on gallium system heterogeneous semiconductor substrate to be prepared from.This gallium oxide film has excellent crystalline quality (because this method first generates one deck gallium oxide on gallium based semiconductor surface, then carry out epitaxial growth again and belong to homoepitaxy, the stress that basic elimination lattice mismatch causes, and then the defect caused is just few), can well and other semi-conducting material carry out combination collocation, make gallium oxide film can have more wide application.
The present invention is further illustrated below by way of specific embodiment.
Embodiment 1
Fig. 1 utilizes oxygen ion beam to the schematic diagram of gallium nitride/sapphire compound substrate modifying surface structure again in embodiment 1; Fig. 2 be adopt metal-organic chemical vapor deposition equipment technology to cross at surface modification in embodiment 1 substrate on carry out the schematic diagram of gallium oxide film extension; Fig. 3 is the X-ray diffraction test collection of illustrative plates of the gallium oxide film of preparation in embodiment 1.
Referring to Fig. 1 and Fig. 2, present embodiment discloses a kind of method utilizing metal-organic chemical vapor deposition equipment to prepare gallium oxide film in sapphire 3/ gallium nitride 2 compound substrate, the method adopts energy to be oxygen plasma, specifically comprises following steps:
Step 1: the extension compound substrate of gallium nitride 2 layers on choice for use sapphire 3 substrate, cleared up by substrate surface, mainly for the organic of adsorption and inorganic impurity, and the non-group that substrate surface covers because of reaction divides compound layer; Manner of cleaning up comprises chemistry and physics two kinds.
Step 2: at room temperature, under oxygen plasma 1 environment, bombards compound substrate, wherein oxygen flow 20sccm, and power is 50W, and reative cell pressure is 0.5Pa, and action time is 300s.Make the gallium nitrogen bond fission on gallium nitride top layer, nitrogen-atoms departs from away, and gallium atom can be combined with oxygen atom, forms gallium oxygen key, thus prepares skim gallium oxide film 5 at gallium nitride substrate surface.The degree of crystallinity of controlled oxidization gallium thin layer, stoichiometric proportion, surface topography and thickness is come by reative cell pressure, oxygen plasma action time and bombardment power.
Step 3: pass into gallium source and oxygen source 4, utilize metal-organic chemical vapor deposition equipment, the compound substrate prepared through above-mentioned two steps continues epitaxial growth gallium oxide film.Adjustment trimethyl gallium source temperature is-10 DEG C, source bottle pressure is 800torr and carrier gas (high-purity argon gas) flow 20sccm, and auxiliary gas (high-purity argon gas) flow is 500sccm; Adjustment oxygen flow is 900sccm; Controlling growth temperature is 700 DEG C, and the speed of growth is 0.4 μm/h, grows 1 hour, and sheet is got in then shutdown system cooling, namely obtains the gallium oxide film prepared.
Characterize the gallium oxide film that the present embodiment prepares, the X-ray diffraction test result of sample as shown in Figure 3, tentatively can see that from figure gallium oxide film has (-202) orientation.
Embodiment 2
Fig. 4 utilizes heat radiation method to the schematic diagram of gallium nitride/sapphire compound substrate modifying surface structure again in embodiment 2; Fig. 5 adopts metal-organic chemical vapor deposition equipment technology to cross schematic diagram substrate carrying out gallium oxide film extension at surface modification in embodiment 2; Fig. 6 is the X-ray diffraction test collection of illustrative plates of the gallium oxide film of preparation in embodiment 2.
Referring to Fig. 4 and Fig. 5, present embodiment discloses a kind of method utilizing metal-organic chemical vapor deposition equipment to prepare gallium oxide film in sapphire 3/ gallium nitride 2 compound substrate, the method adopts energy to be thermal radiation, specifically comprises following steps:
Step 1: the extension compound substrate of gallium nitride 2 layers on choice for use sapphire 3 substrate, cleared up by substrate surface, mainly for the organic of adsorption and inorganic impurity, and the non-group that substrate surface covers because of reaction divides compound layer; Manner of cleaning up comprises chemistry and physics two kinds.
Step 2: sapphire 3/ gallium nitride 2 compound substrate is put into thermal annealing stove, under 750 DEG C of high purity oxygen gas atmosphere, carry out 30min heat treatment 6, the gallium nitrogen bond fission on gallium nitride 2 top layer, nitrogen-atoms departs from away, gallium atom can be combined with oxygen atom, forms gallium oxygen key, thus prepares skim gallium oxide film 5 at gallium nitride substrate surface.By the degree of crystallinity of pressure, oxygen flow, heat treatment temperature and time controlled oxidization gallium thin layer, stoichiometric proportion, surface topography and thickness.
Step 3: pass into gallium source and oxygen source 4, utilize metal-organic chemical vapor deposition equipment, the compound substrate prepared through above-mentioned two steps continues epitaxial growth gallium oxide film.Adjustment trimethyl gallium source temperature is-10 DEG C, source bottle pressure is 800torr and carrier gas (high-purity argon gas) flow 20sccm, and auxiliary gas (high-purity argon gas) flow is 500sccm; Adjustment oxygen flow is 900sccm; Controlling growth temperature is 700 DEG C, and the speed of growth is 0.4 μm/h, grows 1 hour, and sheet is got in then shutdown system cooling, namely obtains the gallium oxide film prepared.
Characterize the gallium oxide film that the present embodiment prepares, as shown in Figure 6, gallium oxide film has (-402) orientation to the X-ray diffraction test result of sample as we can see from the figure.
The present invention is not limited on gallium system heterogeneous semiconductor substrate, prepare gallium oxide film method and gallium oxide film described in above-described embodiment, the change of substrate cleaning way, the change of energy kind, prepares the change of gallium oxide film method or reaction condition all within protection scope of the present invention.
Last it is noted that above each embodiment is only in order to illustrate technical scheme of the present invention, be not intended to limit; Although with reference to foregoing embodiments to invention has been detailed description, those of ordinary skill in the art is to be understood that: it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein some or all of technical characteristic; And these amendments or replacement, do not make the essence of appropriate technical solution depart from the scope of various embodiments of the present invention technical scheme.
Claims (10)
1. on gallium system heterogeneous semiconductor substrate, prepare a method for gallium oxide film, it is characterized in that, comprise the following steps:
Step 1) choose gallium based semiconductor substrate, and clear up gallium based semiconductor substrate surface;
Step 2) containing in the atmosphere of partial pressure of oxygen, external energy is adopted to process gallium based semiconductor substrate, the chemical bond that the gallium atom of gallium based semiconductor substrate surface area and other constituent atoms are formed is opened, the oxygen atom of gallium atom in atmosphere is combined and forms gallium oxygen key;
Step 3) adopt gallium oxide film growing technology gallium based semiconductor Grown gallium oxide film after treatment.
2. on gallium system heterogeneous semiconductor substrate, prepare the method for gallium oxide film according to claim 1, it is characterized in that, described cleaning gallium based semiconductor substrate surface is the organic and inorganic impurity removing the absorption of gallium based semiconductor substrate surface, and the compound layer that substrate surface covers because of reaction.
3. on gallium system heterogeneous semiconductor substrate, prepare the method for gallium oxide film according to claim 1, it is characterized in that, described manner of cleaning up comprises chemical cleaning and/or physical cleaning.
4. on gallium system heterogeneous semiconductor substrate, prepare the method for gallium oxide film according to claim 1, it is characterized in that, described energy is one or more in ion beam bombardment, high energy particle irradiation, electromagnetic field and thermal radiation.
5. on gallium system heterogeneous semiconductor substrate, prepare the method for gallium oxide film according to claim 1, it is characterized in that, described step 2) temperature 50-1200 DEG C of regulation and control process, air pressure is 10
-2-10
3torr, time is 1-120min, the intensity of energy is equivalent to as each gallium atom of substrate surface provides energy 10
-1-10
2eV.
6. on gallium system heterogeneous semiconductor substrate, prepare the method for gallium oxide film according to claim 1, it is characterized in that, described gallium oxide film growing technology is the gallium oxide film growing technology of controlled extension speed.
7. on gallium system heterogeneous semiconductor substrate, prepare the method for gallium oxide film according to claim 6, it is characterized in that, the control precision of the gallium oxide film growing technology of described controlled extension speed reaches atomic layer rank.
8. according to claim 1 or 6, on gallium system heterogeneous semiconductor substrate, prepare the method for gallium oxide film, it is characterized in that, described gallium oxide film growing technology is the one in magnetron sputtering, atomic layer epitaxy, molecular beam epitaxy and metal-organic chemical vapor deposition equipment technology.
9. on gallium system heterogeneous semiconductor substrate, prepare the method for gallium oxide film according to claim 1, it is characterized in that, described step 3) temperature be 300-1200 DEG C, reative cell air pressure is 10
-9-10
3torr, oxygen source are 10 with the molar flow ratio in gallium source
-1-10
5.
10. a gallium oxide film, is characterized in that, adopts the method preparing gallium oxide film described in claim 1-9 any one on gallium system heterogeneous semiconductor substrate to be prepared from.
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| CN106711020B (en) * | 2015-11-18 | 2021-09-17 | 北京北方华创微电子装备有限公司 | Nitridation method of substrate and preparation method of gallium nitride buffer layer |
| CN107785241B (en) * | 2017-10-09 | 2019-08-02 | 哈尔滨工业大学 | A method of preparing beta-gallium oxide film on a silicon substrate |
| CN110504343B (en) * | 2018-05-18 | 2021-02-23 | 中国科学院苏州纳米技术与纳米仿生研究所 | Gallium oxide film based on sapphire substrate and growth method and application thereof |
| CN109346400B (en) * | 2018-10-17 | 2021-09-10 | 吉林大学 | High-quality Ga2O3Film and heteroepitaxial preparation method thereof |
| CN110752158A (en) * | 2019-10-28 | 2020-02-04 | 中国科学技术大学 | Method for repairing surface defects of gallium oxide material |
| CN111128687B (en) * | 2019-12-30 | 2022-05-06 | 镓特半导体科技（上海）有限公司 | Preparation method of self-supporting gallium nitride layer |
| TR202019031A2 (en) * | 2020-11-25 | 2021-02-22 | Univ Yildiz Teknik | High quality hetero epitaxial monoclinic gallium oxide crystal growth method |
| CN115863149B (en) * | 2022-12-12 | 2023-07-21 | 中国科学院上海微系统与信息技术研究所 | Preparation method of gallium oxide structure |
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| CN1833310A (en) * | 2003-08-08 | 2006-09-13 | 株式会社光波 | Semiconductor layer |
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